# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Heterobimetallic peroxo-titanium(IV) nitrilotriacetate complexes as single source precursors for preparation of MTiO3 (M = Co, Ni and Zn) ; _publ_contact_author_name 'Yuanfu Deng' _publ_contact_author_email CHYFDENG@GMAIL.COM loop_ _publ_author_name 'Yuanfu Deng' 'Qi-ying Lv' 'Songping Wu' 'Shuzhong Zhan' # Attachment 'cif1-3.cif' #------------------------------------------------------------------------------ data_1 _database_code_depnum_ccdc_archive 'CCDC 749596' #TrackingRef 'cif1-3.cif' #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H46 Co2 N2 O34 Ti2' _chemical_formula_weight 976.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.015(3) _cell_length_b 13.233(3) _cell_length_c 17.495(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.01(3) _cell_angle_gamma 90.00 _cell_volume 3412.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 1.530 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16365 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3905 _reflns_number_gt 3140 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+1.5827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3905 _refine_ls_number_parameters 287 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0979 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.13311(2) 0.38409(3) 0.467846(19) 0.02333(11) Uani 1 1 d . . . Ti1 Ti 0.42354(3) 0.36188(3) 0.31853(2) 0.01718(12) Uani 1 1 d . . . C1 C 0.21932(17) 0.34188(19) 0.24536(14) 0.0236(5) Uani 1 1 d . . . H1A H 0.1898 0.2782 0.2288 0.028 Uiso 1 1 calc R . . H1B H 0.1795 0.3959 0.2221 0.028 Uiso 1 1 calc R . . C2 C 0.23196(16) 0.34952(17) 0.33261(14) 0.0197(5) Uani 1 1 d . . . C3 C 0.32217(18) 0.25506(18) 0.17444(13) 0.0233(5) Uani 1 1 d . . . H3A H 0.3635 0.2697 0.1395 0.028 Uiso 1 1 calc R . . H3B H 0.2656 0.2307 0.1435 0.028 Uiso 1 1 calc R . . C4 C 0.36255(17) 0.17510(18) 0.23204(14) 0.0233(5) Uani 1 1 d . . . C5 C 0.30852(18) 0.43943(18) 0.16876(13) 0.0238(5) Uani 1 1 d . . . H5A H 0.2491 0.4520 0.1371 0.029 Uiso 1 1 calc R . . H5B H 0.3512 0.4294 0.1342 0.029 Uiso 1 1 calc R . . C6 C 0.33742(18) 0.52951(18) 0.22089(14) 0.0244(5) Uani 1 1 d . . . N1 N 0.30521(13) 0.34805(14) 0.21629(11) 0.0175(4) Uani 1 1 d . . . O1 O 0.31157(12) 0.35835(14) 0.37131(10) 0.0265(4) Uani 1 1 d . . . O2 O 0.16255(12) 0.34691(14) 0.36094(10) 0.0267(4) Uani 1 1 d . . . O3 O 0.39883(12) 0.20605(13) 0.30016(9) 0.0246(4) Uani 1 1 d . . . O4 O 0.36121(14) 0.08618(14) 0.21027(11) 0.0346(5) Uani 1 1 d . . . O5 O 0.38303(12) 0.50952(13) 0.28928(10) 0.0267(4) Uani 1 1 d . . . O6 O 0.32093(16) 0.61549(14) 0.19566(12) 0.0395(5) Uani 1 1 d . . . O7 O 0.5000 0.36131(18) 0.2500 0.0226(5) Uani 1 2 d S . . O8 O 0.49888(12) 0.31442(14) 0.41069(9) 0.0262(4) Uani 1 1 d . . . O9 O 0.49299(13) 0.42563(14) 0.40663(10) 0.0282(4) Uani 1 1 d . . . O1W O 0.08803(18) 0.41714(17) 0.57056(11) 0.0430(6) Uani 1 1 d D . . O2W O 0.25785(14) 0.36834(16) 0.53667(12) 0.0362(5) Uani 1 1 d D . . O3W O 0.17279(14) 0.53790(15) 0.44742(11) 0.0335(4) Uani 1 1 d D . . O4W O 0.09052(13) 0.23437(14) 0.47624(10) 0.0282(4) Uani 1 1 d D . . O5W O 0.00253(13) 0.41421(15) 0.40300(10) 0.0287(4) Uani 1 1 d D . . O6W O 0.0000 0.4536(2) 0.2500 0.0336(6) Uani 1 2 d SD . . O7W O 0.12794(17) 0.30516(19) 0.05056(13) 0.0468(5) Uani 1 1 d D . . O8W O 0.35895(17) 0.5769(2) 0.46179(14) 0.0525(6) Uani 1 1 d D . . O9W O 0.49446(19) 0.6859(2) 0.33733(14) 0.0552(6) Uani 1 1 d D . . H1W1 H 0.057(2) 0.4687(17) 0.576(2) 0.066 Uiso 1 1 d D . . H1W2 H 0.087(3) 0.374(2) 0.6057(17) 0.066 Uiso 1 1 d D . . H2W1 H 0.2998(16) 0.334(2) 0.524(2) 0.066 Uiso 1 1 d D . . H2W2 H 0.2109(15) 0.335(2) 0.537(2) 0.066 Uiso 1 1 d D . . H3W1 H 0.2299(8) 0.543(3) 0.4627(18) 0.066 Uiso 1 1 d D . . H3W2 H 0.159(2) 0.555(3) 0.4001(9) 0.066 Uiso 1 1 d D . . H4W1 H 0.062(2) 0.220(3) 0.5129(13) 0.066 Uiso 1 1 d D . . H4W2 H 0.056(2) 0.215(3) 0.4332(12) 0.066 Uiso 1 1 d D . . H5W1 H -0.036(2) 0.372(2) 0.4133(19) 0.066 Uiso 1 1 d D . . H5W2 H 0.008(3) 0.410(3) 0.3560(9) 0.066 Uiso 1 1 d D . . H6W1 H 0.0459(18) 0.491(3) 0.261(2) 0.066 Uiso 1 1 d D . . H7W1 H 0.129(3) 0.332(2) 0.0072(15) 0.066 Uiso 1 1 d D . . H7W2 H 0.117(3) 0.2424(14) 0.045(2) 0.066 Uiso 1 1 d D . . H8W1 H 0.394(2) 0.556(3) 0.5020(13) 0.066 Uiso 1 1 d D . . H8W2 H 0.373(3) 0.552(3) 0.4215(13) 0.066 Uiso 1 1 d D . . H9W1 H 0.458(2) 0.636(2) 0.327(2) 0.066 Uiso 1 1 d D . . H9W2 H 0.530(2) 0.689(3) 0.3049(17) 0.066 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0259(2) 0.02373(19) 0.02083(19) 0.00126(12) 0.00566(14) 0.00273(13) Ti1 0.0173(2) 0.0197(2) 0.0148(2) -0.00049(14) 0.00385(16) -0.00009(15) C1 0.0193(12) 0.0286(13) 0.0232(12) -0.0007(9) 0.0047(10) -0.0014(10) C2 0.0181(11) 0.0188(11) 0.0229(12) 0.0008(8) 0.0060(9) 0.0017(9) C3 0.0289(13) 0.0206(12) 0.0197(12) -0.0033(9) 0.0026(10) 0.0048(10) C4 0.0245(13) 0.0205(12) 0.0251(13) -0.0005(9) 0.0057(10) 0.0017(10) C5 0.0297(13) 0.0206(12) 0.0204(12) 0.0040(9) 0.0035(10) -0.0008(10) C6 0.0269(13) 0.0215(12) 0.0254(13) 0.0009(9) 0.0066(10) -0.0018(10) N1 0.0193(10) 0.0166(9) 0.0173(9) -0.0006(7) 0.0051(8) 0.0012(7) O1 0.0225(9) 0.0407(11) 0.0174(9) -0.0009(7) 0.0061(7) -0.0011(8) O2 0.0244(9) 0.0350(10) 0.0222(9) -0.0021(7) 0.0082(7) -0.0003(8) O3 0.0313(10) 0.0204(8) 0.0206(8) 0.0016(6) 0.0009(7) -0.0004(7) O4 0.0454(12) 0.0204(9) 0.0345(10) -0.0056(7) -0.0014(9) 0.0063(8) O5 0.0323(10) 0.0194(9) 0.0264(9) -0.0016(7) 0.0002(7) 0.0009(7) O6 0.0558(14) 0.0190(9) 0.0390(12) 0.0056(8) -0.0030(10) -0.0010(9) O7 0.0206(12) 0.0292(13) 0.0195(12) 0.000 0.0077(10) 0.000 O8 0.0271(10) 0.0303(10) 0.0202(9) 0.0035(7) 0.0020(7) 0.0006(7) O9 0.0305(10) 0.0300(10) 0.0228(9) -0.0050(7) 0.0016(7) -0.0037(8) O1W 0.0681(16) 0.0368(12) 0.0299(11) 0.0100(8) 0.0237(10) 0.0231(11) O2W 0.0272(10) 0.0464(12) 0.0327(11) -0.0045(9) -0.0003(9) 0.0086(9) O3W 0.0404(11) 0.0290(10) 0.0301(10) 0.0037(8) 0.0046(8) -0.0013(9) O4W 0.0332(10) 0.0279(9) 0.0237(9) 0.0029(7) 0.0061(8) -0.0002(8) O5W 0.0260(10) 0.0322(10) 0.0286(10) 0.0038(7) 0.0071(8) 0.0056(8) O6W 0.0295(15) 0.0320(15) 0.0364(15) 0.000 -0.0008(12) 0.000 O7W 0.0451(13) 0.0484(14) 0.0477(13) -0.0011(10) 0.0110(11) -0.0002(11) O8W 0.0421(14) 0.0672(17) 0.0458(13) -0.0202(12) 0.0022(11) 0.0036(12) O9W 0.0594(17) 0.0600(16) 0.0446(14) -0.0125(11) 0.0056(12) -0.0200(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2W 2.035(2) . ? Co1 O2 2.0619(18) . ? Co1 O1W 2.0839(19) . ? Co1 O4W 2.0956(19) . ? Co1 O5W 2.107(2) . ? Co1 O3W 2.169(2) . ? Ti1 O7 1.8113(6) . ? Ti1 O9 1.8872(17) . ? Ti1 O8 1.8914(18) . ? Ti1 O1 2.0675(19) . ? Ti1 O5 2.0810(18) 1 ? Ti1 O5 2.0810(18) . ? Ti1 O3 2.1089(18) . ? Ti1 N1 2.275(2) . ? C1 N1 1.476(3) . ? C1 C2 1.505(3) . ? C2 O2 1.237(3) . ? C2 O1 1.262(3) . ? C3 N1 1.479(3) . ? C3 C4 1.506(3) . ? C4 O4 1.236(3) . ? C4 O3 1.279(3) . ? C5 N1 1.474(3) . ? C5 C6 1.513(3) . ? C6 O6 1.228(3) . ? C6 O5 1.288(3) 1 ? C6 O5 1.288(3) . ? O5 O5 0.000(5) 1 ? O7 Ti1 1.8113(6) 2_655 ? O8 O9 1.475(3) . ? O6W O6W 0.0000 1 ? O8W O8W 0.000(10) 1 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2W Co1 O2 100.36(8) . . ? O2W Co1 O1W 85.70(10) . . ? O2 Co1 O1W 173.43(9) . . ? O2W Co1 O4W 96.92(8) . . ? O2 Co1 O4W 87.66(7) . . ? O1W Co1 O4W 89.10(8) . . ? O2W Co1 O5W 174.08(8) . . ? O2 Co1 O5W 83.99(8) . . ? O1W Co1 O5W 90.15(9) . . ? O4W Co1 O5W 87.23(8) . . ? O2W Co1 O3W 86.72(8) . . ? O2 Co1 O3W 87.78(8) . . ? O1W Co1 O3W 95.15(8) . . ? O4W Co1 O3W 174.61(7) . . ? O5W Co1 O3W 89.45(8) . . ? O7 Ti1 O9 102.78(7) . . ? O7 Ti1 O8 102.20(7) . . ? O9 Ti1 O8 45.96(8) . . ? O7 Ti1 O1 165.41(5) . . ? O9 Ti1 O1 90.85(8) . . ? O8 Ti1 O1 90.96(8) . . ? O7 Ti1 O5 91.93(9) . 1 ? O9 Ti1 O5 82.59(8) . 1 ? O8 Ti1 O5 128.35(7) . 1 ? O1 Ti1 O5 84.64(8) . 1 ? O7 Ti1 O5 91.93(9) . . ? O9 Ti1 O5 82.59(8) . . ? O8 Ti1 O5 128.35(7) . . ? O1 Ti1 O5 84.64(8) . . ? O5 Ti1 O5 0.00(14) 1 . ? O7 Ti1 O3 90.59(9) . . ? O9 Ti1 O3 127.98(7) . . ? O8 Ti1 O3 82.21(7) . . ? O1 Ti1 O3 84.93(7) . . ? O5 Ti1 O3 147.77(7) 1 . ? O5 Ti1 O3 147.77(7) . . ? O7 Ti1 N1 88.73(5) . . ? O9 Ti1 N1 154.81(8) . . ? O8 Ti1 N1 153.35(8) . . ? O1 Ti1 N1 76.69(7) . . ? O5 Ti1 N1 74.60(7) 1 . ? O5 Ti1 N1 74.60(7) . . ? O3 Ti1 N1 73.34(7) . . ? N1 C1 C2 113.4(2) . . ? O2 C2 O1 124.9(2) . . ? O2 C2 C1 116.9(2) . . ? O1 C2 C1 118.3(2) . . ? N1 C3 C4 109.80(19) . . ? O4 C4 O3 124.8(2) . . ? O4 C4 C3 118.8(2) . . ? O3 C4 C3 116.3(2) . . ? N1 C5 C6 110.06(19) . . ? O6 C6 O5 124.0(2) . 1 ? O6 C6 O5 124.0(2) . . ? O5 C6 O5 0.00(17) 1 . ? O6 C6 C5 119.9(2) . . ? O5 C6 C5 116.0(2) 1 . ? O5 C6 C5 116.0(2) . . ? C5 N1 C1 111.44(19) . . ? C5 N1 C3 112.08(18) . . ? C1 N1 C3 111.65(19) . . ? C5 N1 Ti1 105.80(14) . . ? C1 N1 Ti1 109.64(14) . . ? C3 N1 Ti1 105.89(14) . . ? C2 O1 Ti1 122.03(16) . . ? C2 O2 Co1 134.41(16) . . ? C4 O3 Ti1 119.09(15) . . ? O5 O5 C6 0(10) 1 . ? O5 O5 Ti1 0(10) 1 . ? C6 O5 Ti1 120.00(15) . . ? Ti1 O7 Ti1 179.52(15) . 2_655 ? O9 O8 Ti1 66.87(9) . . ? O8 O9 Ti1 67.17(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W2 O3 0.841(10) 1.936(13) 2.764(3) 168(4) 7_556 O1W H1W1 O5W 0.842(10) 1.860(11) 2.699(3) 174(4) 5_566 O2W H2W1 O4W 0.840(10) 1.880(14) 2.698(3) 164(4) 7_556 O3W H3W2 O4 0.847(10) 1.940(12) 2.782(3) 173(4) 4 O3W H3W1 O8W 0.852(10) 1.991(16) 2.806(3) 160(3) 1 O4W H4W1 O8 0.855(18) 1.819(18) 2.673(3) 178(4) 7_556 O4W H4W2 O9W 0.870(17) 1.794(17) 2.657(3) 172(3) 3_445 O5W H5W2 O6W 0.842(10) 1.926(18) 2.720(2) 157(4) 1 O5W H5W1 O7W 0.850(10) 1.849(13) 2.681(3) 166(4) 2 O6W H6W1 O4 0.844(10) 1.872(11) 2.711(3) 173(4) 4 O7W H7W1 O3W 0.842(18) 2.18(2) 2.913(3) 146(3) 6_565 O7W H7W2 O8W 0.848(17) 2.22(2) 3.037(4) 160(4) 4_545 O8W H8W1 O9 0.838(17) 2.11(3) 2.879(3) 151(4) 5_666 O9W H9W1 O5 0.848(10) 2.061(13) 2.902(3) 171(3) 1 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.542 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.111 #===END #------------------------------------------------------------------------------ data_2 _database_code_depnum_ccdc_archive 'CCDC 749597' #TrackingRef 'cif1-3.cif' #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H46 N2 Ni2 O34 Ti2' _chemical_formula_weight 975.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.043(3) _cell_length_b 13.250(3) _cell_length_c 17.368(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.92(3) _cell_angle_gamma 90.00 _cell_volume 3399.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour gree _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 1.668 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15938 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3884 _reflns_number_gt 3352 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+3.7381P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3884 _refine_ls_number_parameters 287 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.13279(2) 0.38547(2) 0.467622(17) 0.02249(11) Uani 1 1 d . . . Ti1 Ti 0.42326(3) 0.36081(3) 0.31894(2) 0.01732(11) Uani 1 1 d . . . C1 C 0.21895(16) 0.34116(18) 0.24551(13) 0.0222(5) Uani 1 1 d . . . H1A H 0.1898 0.2773 0.2293 0.027 Uiso 1 1 calc R . . H1B H 0.1790 0.3947 0.2217 0.027 Uiso 1 1 calc R . . C2 C 0.23165(16) 0.35001(16) 0.33359(13) 0.0197(4) Uani 1 1 d . . . C3 C 0.32164(16) 0.25436(17) 0.17399(13) 0.0226(5) Uani 1 1 d . . . H3A H 0.3626 0.2689 0.1385 0.027 Uiso 1 1 calc R . . H3B H 0.2651 0.2300 0.1432 0.027 Uiso 1 1 calc R . . C4 C 0.36240(16) 0.17433(17) 0.23215(14) 0.0223(5) Uani 1 1 d . . . C5 C 0.30834(17) 0.43865(17) 0.16827(13) 0.0241(5) Uani 1 1 d . . . H5A H 0.2490 0.4514 0.1366 0.029 Uiso 1 1 calc R . . H5B H 0.3507 0.4285 0.1333 0.029 Uiso 1 1 calc R . . C6 C 0.33764(16) 0.52864(17) 0.22092(14) 0.0239(5) Uani 1 1 d . . . N1 N 0.30505(13) 0.34731(13) 0.21615(10) 0.0174(4) Uani 1 1 d . . . O1 O 0.31115(11) 0.35841(14) 0.37243(10) 0.0263(4) Uani 1 1 d . . . O2 O 0.16186(11) 0.34870(13) 0.36177(10) 0.0258(4) Uani 1 1 d . . . O3 O 0.39829(12) 0.20482(12) 0.30064(9) 0.0240(3) Uani 1 1 d . . . O4 O 0.36124(14) 0.08520(13) 0.20998(11) 0.0341(4) Uani 1 1 d . . . O5 O 0.38352(12) 0.50906(12) 0.28956(10) 0.0260(4) Uani 1 1 d . . . O6 O 0.32087(16) 0.61470(13) 0.19536(12) 0.0397(5) Uani 1 1 d . . . O7 O 0.5000 0.35963(18) 0.2500 0.0234(5) Uani 1 2 d S . . O8 O 0.49874(11) 0.31305(13) 0.41168(10) 0.0264(4) Uani 1 1 d . . . O9 O 0.49304(12) 0.42409(14) 0.40780(10) 0.0291(4) Uani 1 1 d . . . O1W O 0.08926(17) 0.41898(16) 0.56907(11) 0.0422(5) Uani 1 1 d D . . O2W O 0.25569(14) 0.36747(16) 0.53436(11) 0.0361(4) Uani 1 1 d D . . O3W O 0.17185(13) 0.53616(14) 0.44898(11) 0.0317(4) Uani 1 1 d D . . O4W O 0.09295(12) 0.23775(13) 0.47601(10) 0.0273(4) Uani 1 1 d D . . O5W O 0.00389(12) 0.41498(14) 0.40427(10) 0.0285(4) Uani 1 1 d D . . O6W O 0.0000 0.4535(2) 0.2500 0.0320(6) Uani 1 2 d SD . . O7W O 0.12707(16) 0.30502(18) 0.05071(14) 0.0466(5) Uani 1 1 d D . . O8W O 0.35762(16) 0.5775(2) 0.46113(15) 0.0529(6) Uani 1 1 d D . . O9W O 0.49562(19) 0.6858(2) 0.33713(15) 0.0574(6) Uani 1 1 d D . . H1W1 H 0.060(2) 0.4711(16) 0.576(2) 0.069 Uiso 1 1 d D . . H1W2 H 0.085(3) 0.3735(19) 0.6019(19) 0.069 Uiso 1 1 d D . . H2W1 H 0.2994(19) 0.338(3) 0.5199(19) 0.069 Uiso 1 1 d D . . H2W2 H 0.262(3) 0.368(3) 0.5834(7) 0.069 Uiso 1 1 d D . . H3W1 H 0.2282(9) 0.544(3) 0.4650(19) 0.069 Uiso 1 1 d D . . H3W2 H 0.158(2) 0.554(3) 0.4009(9) 0.069 Uiso 1 1 d D . . H4W1 H 0.069(2) 0.218(3) 0.5147(14) 0.069 Uiso 1 1 d D . . H4W2 H 0.059(2) 0.217(3) 0.4337(12) 0.069 Uiso 1 1 d D . . H5W1 H -0.031(2) 0.368(2) 0.415(2) 0.069 Uiso 1 1 d D . . H5W2 H 0.010(3) 0.409(3) 0.3571(10) 0.069 Uiso 1 1 d D . . H6W1 H 0.0428(18) 0.495(2) 0.262(3) 0.069 Uiso 1 1 d D . . H7W1 H 0.128(3) 0.333(2) 0.0081(16) 0.069 Uiso 1 1 d D . . H7W2 H 0.122(3) 0.2419(13) 0.046(2) 0.069 Uiso 1 1 d D . . H8W1 H 0.391(2) 0.555(3) 0.5016(13) 0.069 Uiso 1 1 d D . . H8W2 H 0.373(3) 0.558(3) 0.4201(13) 0.069 Uiso 1 1 d D . . H9W1 H 0.460(2) 0.637(2) 0.325(2) 0.069 Uiso 1 1 d D . . H9W2 H 0.522(2) 0.701(3) 0.2996(15) 0.069 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02372(18) 0.02516(17) 0.01921(17) 0.00146(11) 0.00567(12) 0.00311(12) Ti1 0.0163(2) 0.0214(2) 0.0149(2) -0.00018(14) 0.00470(15) -0.00006(14) C1 0.0178(11) 0.0304(12) 0.0185(11) -0.0018(9) 0.0040(9) -0.0014(9) C2 0.0205(11) 0.0192(10) 0.0205(11) 0.0000(8) 0.0065(9) 0.0011(8) C3 0.0273(12) 0.0232(11) 0.0169(10) -0.0048(8) 0.0031(9) 0.0025(9) C4 0.0208(11) 0.0213(11) 0.0251(12) -0.0013(9) 0.0050(9) 0.0003(9) C5 0.0308(12) 0.0229(11) 0.0185(11) 0.0042(8) 0.0044(9) -0.0029(9) C6 0.0252(12) 0.0205(11) 0.0264(12) 0.0023(9) 0.0059(10) -0.0004(9) N1 0.0199(9) 0.0170(8) 0.0161(9) -0.0005(7) 0.0058(7) -0.0001(7) O1 0.0190(8) 0.0432(10) 0.0176(8) -0.0011(7) 0.0058(6) 0.0005(7) O2 0.0210(8) 0.0365(9) 0.0217(8) -0.0024(7) 0.0089(7) 0.0001(7) O3 0.0293(9) 0.0209(8) 0.0205(8) 0.0014(6) 0.0014(7) -0.0004(7) O4 0.0430(11) 0.0220(8) 0.0346(10) -0.0049(7) 0.0005(9) 0.0059(8) O5 0.0302(9) 0.0210(8) 0.0248(9) -0.0012(6) 0.0000(7) 0.0008(7) O6 0.0544(13) 0.0226(9) 0.0375(11) 0.0048(7) -0.0028(10) -0.0003(8) O7 0.0197(11) 0.0317(12) 0.0204(11) 0.000 0.0077(9) 0.000 O8 0.0245(9) 0.0336(9) 0.0202(8) 0.0019(7) 0.0020(7) 0.0008(7) O9 0.0286(9) 0.0347(9) 0.0225(8) -0.0042(7) 0.0010(7) -0.0035(7) O1W 0.0665(15) 0.0381(11) 0.0275(10) 0.0093(8) 0.0232(10) 0.0236(10) O2W 0.0297(10) 0.0505(12) 0.0257(10) -0.0050(8) -0.0011(8) 0.0113(8) O3W 0.0366(10) 0.0291(9) 0.0288(9) 0.0036(7) 0.0052(8) 0.0001(8) O4W 0.0299(9) 0.0290(9) 0.0234(9) 0.0029(7) 0.0066(7) 0.0004(7) O5W 0.0268(9) 0.0330(9) 0.0265(9) 0.0040(7) 0.0070(7) 0.0064(7) O6W 0.0261(13) 0.0358(14) 0.0322(14) 0.000 0.0009(11) 0.000 O7W 0.0419(12) 0.0509(13) 0.0487(13) -0.0017(10) 0.0128(11) 0.0000(11) O8W 0.0411(13) 0.0696(16) 0.0464(13) -0.0202(12) 0.0044(11) 0.0032(11) O9W 0.0589(16) 0.0645(16) 0.0461(14) -0.0121(12) 0.0034(12) -0.0225(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2W 2.002(2) . ? Ni1 O2 2.0282(17) . ? Ni1 O1W 2.0414(19) . ? Ni1 O4W 2.0602(18) . ? Ni1 O5W 2.0772(19) . ? Ni1 O3W 2.1234(19) . ? Ti1 O7 1.8138(6) . ? Ti1 O9 1.8901(18) . ? Ti1 O8 1.8951(18) . ? Ti1 O1 2.0741(17) . ? Ti1 O5 2.0882(17) 1 ? Ti1 O5 2.0882(17) . ? Ti1 O3 2.1140(17) . ? Ti1 N1 2.276(2) . ? C1 N1 1.481(3) . ? C1 C2 1.510(3) . ? C2 O2 1.239(3) . ? C2 O1 1.262(3) . ? C3 N1 1.478(3) . ? C3 C4 1.512(3) . ? C4 O4 1.241(3) . ? C4 O3 1.275(3) . ? C5 N1 1.475(3) . ? C5 C6 1.516(3) . ? C6 O6 1.232(3) . ? C6 O5 1.286(3) 1 ? C6 O5 1.286(3) . ? O5 O5 0.000(6) 1 ? O7 Ti1 1.8138(6) 2_655 ? O8 O9 1.475(3) . ? O6W O6W 0.000(5) 1 ? O8W O8W 0.000(9) 1 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2W Ni1 O2 99.33(8) . . ? O2W Ni1 O1W 86.46(9) . . ? O2 Ni1 O1W 173.79(9) . . ? O2W Ni1 O4W 95.45(8) . . ? O2 Ni1 O4W 87.22(7) . . ? O1W Ni1 O4W 90.03(8) . . ? O2W Ni1 O5W 175.04(8) . . ? O2 Ni1 O5W 84.55(7) . . ? O1W Ni1 O5W 89.79(9) . . ? O4W Ni1 O5W 87.79(7) . . ? O2W Ni1 O3W 87.04(8) . . ? O2 Ni1 O3W 88.52(7) . . ? O1W Ni1 O3W 94.04(8) . . ? O4W Ni1 O3W 175.36(7) . . ? O5W Ni1 O3W 89.98(8) . . ? O7 Ti1 O9 102.62(7) . . ? O7 Ti1 O8 101.80(6) . . ? O9 Ti1 O8 45.85(8) . . ? O7 Ti1 O1 165.62(5) . . ? O9 Ti1 O1 90.80(8) . . ? O8 Ti1 O1 91.22(7) . . ? O7 Ti1 O5 92.03(9) . 1 ? O9 Ti1 O5 82.60(8) . 1 ? O8 Ti1 O5 128.28(7) . 1 ? O1 Ti1 O5 84.52(7) . 1 ? O7 Ti1 O5 92.03(9) . . ? O9 Ti1 O5 82.60(8) . . ? O8 Ti1 O5 128.28(7) . . ? O1 Ti1 O5 84.52(7) . . ? O5 Ti1 O5 0.00(14) 1 . ? O7 Ti1 O3 90.54(9) . . ? O9 Ti1 O3 127.72(7) . . ? O8 Ti1 O3 82.07(7) . . ? O1 Ti1 O3 85.18(7) . . ? O5 Ti1 O3 148.04(7) 1 . ? O5 Ti1 O3 148.04(7) . . ? O7 Ti1 N1 88.96(5) . . ? O9 Ti1 N1 154.95(8) . . ? O8 Ti1 N1 153.36(7) . . ? O1 Ti1 N1 76.66(7) . . ? O5 Ti1 N1 74.77(7) 1 . ? O5 Ti1 N1 74.77(7) . . ? O3 Ti1 N1 73.44(6) . . ? N1 C1 C2 113.18(19) . . ? O2 C2 O1 125.3(2) . . ? O2 C2 C1 116.4(2) . . ? O1 C2 C1 118.3(2) . . ? N1 C3 C4 109.79(18) . . ? O4 C4 O3 124.7(2) . . ? O4 C4 C3 118.7(2) . . ? O3 C4 C3 116.57(19) . . ? N1 C5 C6 110.01(18) . . ? O6 C6 O5 123.9(2) . 1 ? O6 C6 O5 123.9(2) . . ? O5 C6 O5 0.00(16) 1 . ? O6 C6 C5 119.6(2) . . ? O5 C6 C5 116.4(2) 1 . ? O5 C6 C5 116.4(2) . . ? C5 N1 C3 112.19(17) . . ? C5 N1 C1 111.37(18) . . ? C3 N1 C1 111.44(18) . . ? C5 N1 Ti1 105.85(14) . . ? C3 N1 Ti1 105.90(13) . . ? C1 N1 Ti1 109.78(13) . . ? C2 O1 Ti1 122.06(15) . . ? C2 O2 Ni1 134.32(16) . . ? C4 O3 Ti1 118.80(14) . . ? O5 O5 C6 0(10) 1 . ? O5 O5 Ti1 0(10) 1 . ? C6 O5 Ti1 119.66(14) . . ? Ti1 O7 Ti1 179.01(15) 2_655 . ? O9 O8 Ti1 66.90(9) . . ? O8 O9 Ti1 67.25(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W2 O3 0.840(10) 1.961(17) 2.772(2) 162(4) 7_556 O1W H1W1 O5W 0.836(10) 1.860(11) 2.695(3) 177(3) 5_566 O2W H2W2 O6 0.839(10) 1.993(19) 2.792(3) 159(4) 6_566 O2W H2W1 O4W 0.846(10) 1.891(16) 2.705(3) 161(3) 7_556 O3W H3W2 O4 0.854(10) 1.937(11) 2.788(3) 174(4) 4 O3W H3W1 O8W 0.847(10) 2.010(17) 2.816(3) 159(3) 1 O4W H4W1 O8 0.855(18) 1.83(2) 2.679(3) 170(4) 7_556 O4W H4W2 O9W 0.860(18) 1.811(17) 2.664(3) 172(4) 3_445 O5W H5W2 O6W 0.847(10) 1.93(2) 2.7172(19) 154(4) 1 O5W H5W1 O7W 0.853(10) 1.865(16) 2.683(3) 160(4) 2 O6W H6W1 O4 0.839(10) 1.870(11) 2.709(3) 178(5) 4 O7W H7W1 O3W 0.832(18) 2.18(2) 2.908(3) 146(4) 6_565 O7W H7W2 O8W 0.843(18) 2.21(2) 3.034(4) 167(4) 4_545 O8W H8W1 O9 0.837(18) 2.13(3) 2.880(3) 148(4) 5_666 O9W H9W1 O5 0.842(10) 2.075(12) 2.912(3) 173(4) 1 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.873 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.102 #===END #------------------------------------------------------------------------------ data_3 _database_code_depnum_ccdc_archive 'CCDC 749598' #TrackingRef 'cif1-3.cif' #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H46 N2 O34 Ti2 Zn2' _chemical_formula_weight 989.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.015(3) _cell_length_b 13.233(3) _cell_length_c 17.495(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.01(3) _cell_angle_gamma 90.00 _cell_volume 3412.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.964 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16309 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3915 _reflns_number_gt 2647 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3915 _refine_ls_number_parameters 287 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.13425(3) 0.38310(3) 0.46872(2) 0.02550(14) Uani 1 1 d . . . Ti1 Ti 0.42338(4) 0.36135(5) 0.31874(3) 0.01909(16) Uani 1 1 d . . . C1 C 0.2194(2) 0.3410(3) 0.24615(19) 0.0251(8) Uani 1 1 d . . . H1A H 0.1900 0.2772 0.2297 0.030 Uiso 1 1 calc R . . H1B H 0.1793 0.3948 0.2229 0.030 Uiso 1 1 calc R . . C2 C 0.2320(2) 0.3488(3) 0.33346(19) 0.0211(7) Uani 1 1 d . . . C3 C 0.3222(2) 0.2549(3) 0.17514(18) 0.0228(8) Uani 1 1 d . . . H3A H 0.3637 0.2698 0.1404 0.027 Uiso 1 1 calc R . . H3B H 0.2659 0.2304 0.1440 0.027 Uiso 1 1 calc R . . C4 C 0.3627(2) 0.1744(3) 0.2328(2) 0.0246(8) Uani 1 1 d . . . C5 C 0.3081(2) 0.4379(3) 0.16926(18) 0.0219(7) Uani 1 1 d . . . H5A H 0.2488 0.4502 0.1375 0.026 Uiso 1 1 calc R . . H5B H 0.3508 0.4276 0.1347 0.026 Uiso 1 1 calc R . . C6 C 0.3369(2) 0.5288(3) 0.2205(2) 0.0262(8) Uani 1 1 d . . . N1 N 0.30480(18) 0.3473(2) 0.21659(15) 0.0187(6) Uani 1 1 d . . . O1 O 0.31150(15) 0.3579(2) 0.37186(13) 0.0282(6) Uani 1 1 d . . . O2 O 0.16229(15) 0.3463(2) 0.36181(13) 0.0290(6) Uani 1 1 d . . . O3 O 0.39931(16) 0.2058(2) 0.30077(13) 0.0266(6) Uani 1 1 d . . . O4 O 0.36172(18) 0.0860(2) 0.21132(15) 0.0350(7) Uani 1 1 d . . . O5 O 0.38251(16) 0.5090(2) 0.28920(13) 0.0274(6) Uani 1 1 d . . . O6 O 0.3201(2) 0.6142(2) 0.19575(16) 0.0398(7) Uani 1 1 d . . . O7 O 0.5000 0.3606(3) 0.2500 0.0237(8) Uani 1 2 d S . . O8 O 0.49904(15) 0.3146(2) 0.41107(13) 0.0278(6) Uani 1 1 d . . . O9 O 0.49318(16) 0.4253(2) 0.40645(14) 0.0304(6) Uani 1 1 d . . . O1W O 0.0866(2) 0.4162(3) 0.56917(16) 0.0445(8) Uani 1 1 d D . . O2W O 0.25704(18) 0.3685(2) 0.53690(16) 0.0374(7) Uani 1 1 d D . . O3W O 0.17255(18) 0.5382(2) 0.44700(15) 0.0334(6) Uani 1 1 d D . . O4W O 0.09083(16) 0.2327(2) 0.47539(14) 0.0289(6) Uani 1 1 d D . . O5W O 0.00243(17) 0.4151(2) 0.40388(14) 0.0294(6) Uani 1 1 d D . . O6W O 0.0000 0.4526(3) 0.2500 0.0329(9) Uani 1 2 d SD . . O7W O 0.1281(2) 0.3046(3) 0.05090(18) 0.0469(8) Uani 1 1 d D . . O8W O 0.3592(2) 0.5779(3) 0.46108(19) 0.0534(9) Uani 1 1 d D . . O9W O 0.4936(2) 0.6864(3) 0.33642(18) 0.0561(10) Uani 1 1 d D . . H1W1 H 0.058(3) 0.469(2) 0.576(3) 0.067 Uiso 1 1 d D . . H1W2 H 0.092(3) 0.377(3) 0.6081(18) 0.067 Uiso 1 1 d D . . H2W1 H 0.300(2) 0.340(4) 0.520(2) 0.067 Uiso 1 1 d D . . H2W2 H 0.267(3) 0.368(4) 0.5860(6) 0.067 Uiso 1 1 d D . . H3W1 H 0.2289(10) 0.543(4) 0.466(2) 0.067 Uiso 1 1 d D . . H3W2 H 0.161(3) 0.567(4) 0.4026(15) 0.067 Uiso 1 1 d D . . H4W1 H 0.063(3) 0.219(4) 0.5119(16) 0.067 Uiso 1 1 d D . . H4W2 H 0.061(3) 0.214(4) 0.4323(13) 0.067 Uiso 1 1 d D . . H5W1 H -0.034(3) 0.372(3) 0.417(2) 0.067 Uiso 1 1 d D . . H5W2 H 0.006(3) 0.408(4) 0.3565(10) 0.067 Uiso 1 1 d D . . H6W1 H 0.046(2) 0.491(3) 0.259(3) 0.067 Uiso 1 1 d D . . H7W1 H 0.140(3) 0.332(3) 0.0110(19) 0.067 Uiso 1 1 d D . . H7W2 H 0.121(3) 0.2424(15) 0.047(3) 0.067 Uiso 1 1 d D . . H8W1 H 0.392(3) 0.560(4) 0.5029(14) 0.067 Uiso 1 1 d D . . H8W2 H 0.371(3) 0.544(4) 0.4231(17) 0.067 Uiso 1 1 d D . . H9W1 H 0.464(3) 0.632(2) 0.325(3) 0.067 Uiso 1 1 d D . . H9W2 H 0.526(3) 0.699(4) 0.3029(19) 0.067 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0266(2) 0.0292(3) 0.0209(2) 0.00118(17) 0.00483(17) 0.00348(18) Ti1 0.0179(3) 0.0241(4) 0.0152(3) -0.0008(2) 0.0031(2) 0.0005(2) C1 0.0189(15) 0.034(2) 0.0219(16) -0.0032(15) 0.0019(14) 0.0000(14) C2 0.0209(16) 0.020(2) 0.0226(16) 0.0009(14) 0.0043(14) 0.0005(13) C3 0.0269(17) 0.022(2) 0.0189(15) -0.0031(14) 0.0039(14) 0.0023(14) C4 0.0200(16) 0.026(2) 0.0277(17) -0.0015(16) 0.0052(15) 0.0007(14) C5 0.0274(17) 0.020(2) 0.0181(15) -0.0008(14) 0.0047(14) 0.0010(14) C6 0.0260(17) 0.028(2) 0.0252(17) 0.0024(15) 0.0058(15) -0.0002(15) N1 0.0199(13) 0.0212(17) 0.0157(12) 0.0022(11) 0.0050(11) 0.0013(11) O1 0.0213(12) 0.0445(19) 0.0192(11) -0.0010(11) 0.0048(10) 0.0013(11) O2 0.0219(12) 0.0424(18) 0.0238(12) 0.0003(11) 0.0075(11) -0.0014(11) O3 0.0327(13) 0.0240(15) 0.0208(11) 0.0021(10) -0.0011(11) -0.0016(11) O4 0.0466(15) 0.0205(16) 0.0343(14) -0.0059(12) -0.0012(13) 0.0073(12) O5 0.0312(12) 0.0241(15) 0.0244(12) -0.0020(10) -0.0016(11) 0.0012(11) O6 0.0553(17) 0.0207(16) 0.0387(15) 0.0076(12) -0.0028(14) -0.0001(13) O7 0.0241(16) 0.029(2) 0.0201(16) 0.000 0.0095(14) 0.000 O8 0.0268(12) 0.0320(17) 0.0230(12) 0.0033(11) 0.0006(11) 0.0008(11) O9 0.0309(13) 0.0342(17) 0.0248(12) -0.0041(11) 0.0024(11) -0.0030(11) O1W 0.070(2) 0.040(2) 0.0281(14) 0.0120(13) 0.0211(15) 0.0219(16) O2W 0.0321(14) 0.052(2) 0.0259(13) -0.0045(13) -0.0007(12) 0.0111(13) O3W 0.0385(14) 0.0302(17) 0.0310(13) 0.0042(12) 0.0051(12) 0.0004(12) O4W 0.0312(13) 0.0323(17) 0.0234(12) 0.0017(11) 0.0056(11) 0.0002(12) O5W 0.0294(13) 0.0327(17) 0.0269(12) 0.0072(12) 0.0072(12) 0.0061(11) O6W 0.0249(18) 0.037(3) 0.035(2) 0.000 0.0017(17) 0.000 O7W 0.0424(16) 0.049(2) 0.0502(18) 0.0000(17) 0.0101(15) -0.0030(16) O8W 0.0419(17) 0.066(3) 0.0494(18) -0.0204(18) 0.0023(16) 0.0021(16) O9W 0.058(2) 0.065(3) 0.0424(17) -0.0113(17) 0.0012(16) -0.0205(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2W 2.005(2) . ? Zn1 O2 2.053(3) . ? Zn1 O1W 2.066(3) . ? Zn1 O4W 2.104(3) . ? Zn1 O5W 2.128(2) . ? Zn1 O3W 2.185(3) . ? Ti1 O7 1.8161(8) . ? Ti1 O9 1.885(2) . ? Ti1 O8 1.893(2) . ? Ti1 O1 2.070(3) . ? Ti1 O5 2.083(3) 1 ? Ti1 O5 2.083(3) . ? Ti1 O3 2.103(3) . ? Ti1 N1 2.277(3) . ? C1 N1 1.474(4) . ? C1 C2 1.506(5) . ? C2 O2 1.241(4) . ? C2 O1 1.259(4) . ? C3 N1 1.470(4) . ? C3 C4 1.512(5) . ? C4 O4 1.228(4) . ? C4 O3 1.281(4) . ? C5 N1 1.464(4) . ? C5 C6 1.512(5) . ? C6 O6 1.219(5) . ? C6 O5 1.292(4) 1 ? C6 O5 1.292(4) . ? O5 O5 0.000(7) 1 ? O7 Ti1 1.8161(8) 2_655 ? O8 O9 1.468(4) . ? O6W O6W 0.000(9) 1 ? O8W O8W 0.000(8) 1 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2W Zn1 O2 101.18(11) . . ? O2W Zn1 O1W 86.71(13) . . ? O2 Zn1 O1W 171.71(12) . . ? O2W Zn1 O4W 97.77(12) . . ? O2 Zn1 O4W 86.89(11) . . ? O1W Zn1 O4W 89.54(12) . . ? O2W Zn1 O5W 173.06(12) . . ? O2 Zn1 O5W 83.87(10) . . ? O1W Zn1 O5W 88.49(12) . . ? O4W Zn1 O5W 87.20(10) . . ? O2W Zn1 O3W 87.22(12) . . ? O2 Zn1 O3W 87.59(11) . . ? O1W Zn1 O3W 95.40(13) . . ? O4W Zn1 O3W 173.18(9) . . ? O5W Zn1 O3W 88.24(10) . . ? O7 Ti1 O9 102.55(10) . . ? O7 Ti1 O8 102.15(9) . . ? O9 Ti1 O8 45.72(12) . . ? O7 Ti1 O1 165.53(7) . . ? O9 Ti1 O1 90.98(11) . . ? O8 Ti1 O1 90.91(10) . . ? O7 Ti1 O5 91.98(13) . 1 ? O9 Ti1 O5 82.70(11) . 1 ? O8 Ti1 O5 128.21(11) . 1 ? O1 Ti1 O5 84.62(11) . 1 ? O7 Ti1 O5 91.98(13) . . ? O9 Ti1 O5 82.70(11) . . ? O8 Ti1 O5 128.21(11) . . ? O1 Ti1 O5 84.62(11) . . ? O5 Ti1 O5 0.00(17) 1 . ? O7 Ti1 O3 90.48(13) . . ? O9 Ti1 O3 127.85(10) . . ? O8 Ti1 O3 82.29(10) . . ? O1 Ti1 O3 85.09(11) . . ? O5 Ti1 O3 147.86(9) 1 . ? O5 Ti1 O3 147.86(9) . . ? O7 Ti1 N1 88.80(8) . . ? O9 Ti1 N1 154.90(12) . . ? O8 Ti1 N1 153.55(11) . . ? O1 Ti1 N1 76.74(9) . . ? O5 Ti1 N1 74.51(10) 1 . ? O5 Ti1 N1 74.51(10) . . ? O3 Ti1 N1 73.52(9) . . ? N1 C1 C2 113.7(3) . . ? O2 C2 O1 125.1(3) . . ? O2 C2 C1 116.8(3) . . ? O1 C2 C1 118.1(3) . . ? N1 C3 C4 110.1(3) . . ? O4 C4 O3 124.8(3) . . ? O4 C4 C3 119.2(3) . . ? O3 C4 C3 115.9(3) . . ? N1 C5 C6 110.7(3) . . ? O6 C6 O5 123.7(3) . 1 ? O6 C6 O5 123.7(3) . . ? O5 C6 O5 0.0(3) 1 . ? O6 C6 C5 120.7(3) . . ? O5 C6 C5 115.5(3) 1 . ? O5 C6 C5 115.5(3) . . ? C5 N1 C3 112.0(3) . . ? C5 N1 C1 111.8(3) . . ? C3 N1 C1 112.0(3) . . ? C5 N1 Ti1 105.71(19) . . ? C3 N1 Ti1 105.61(18) . . ? C1 N1 Ti1 109.37(18) . . ? C2 O1 Ti1 122.1(2) . . ? C2 O2 Zn1 133.9(2) . . ? C4 O3 Ti1 119.2(2) . . ? O5 O5 C6 0(10) 1 . ? O5 O5 Ti1 0(10) 1 . ? C6 O5 Ti1 120.0(2) . . ? Ti1 O7 Ti1 179.4(2) 2_655 . ? O9 O8 Ti1 66.88(12) . . ? O8 O9 Ti1 67.40(13) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W2 O3 0.846(10) 1.920(11) 2.765(4) 177(4) 7_556 O1W H1W1 O5W 0.844(10) 1.847(11) 2.690(4) 177(5) 5_566 O2W H2W2 O6 0.844(10) 1.948(18) 2.769(4) 164(5) 6_566 O2W H2W1 O4W 0.847(10) 1.89(2) 2.692(4) 158(4) 7_556 O3W H3W2 O4 0.851(10) 1.97(2) 2.791(4) 161(5) 4 O3W H3W1 O8W 0.850(10) 2.02(2) 2.815(4) 154(4) 1 O4W H4W1 O8 0.845(18) 1.836(19) 2.680(4) 178(5) 7_556 O4W H4W2 O9W 0.835(18) 1.825(19) 2.658(4) 175(5) 3_445 O5W H5W2 O6W 0.845(10) 1.94(2) 2.731(3) 155(5) 1 O5W H5W1 O7W 0.846(10) 1.852(16) 2.683(4) 167(5) 2 O6W H6W1 O4 0.848(10) 1.869(13) 2.711(4) 172(6) 4 O7W H7W1 O3W 0.832(19) 2.16(3) 2.922(5) 152(5) 6_565 O7W H7W2 O8W 0.832(19) 2.21(2) 3.015(5) 164(5) 4_545 O8W H8W1 O9 0.832(18) 2.12(3) 2.886(4) 153(5) 5_666 O9W H9W1 O5 0.847(10) 2.062(12) 2.906(4) 175(5) 1 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.920 _refine_diff_density_min -1.240 _refine_diff_density_rms 0.177 #===END